Oxygen-deficient wrinkled MxMg1-x oxide antibacterial material as well as preparation and application thereof

Abstract

The invention belongs to the field of antibacterial materials, and particularly relates to an oxygen defect wrinkled MxMg1-x oxide antibacterial material and preparation and application thereof.The preparation method comprises the steps that a metal solution with an Mg source and an M source dispersed is obtained and then subjected to atomization treatment, and metal raw material particles are obtained; the metal raw material particles are subjected to first-stage calcination in an oxygen-free atmosphere at the temperature of 500-1000 DEG C, and then the oxygen-deficient wrinkled MxMg1-x oxide antibacterial material is prepared in an oxygen-containing atmosphere; in the M < x > Mg < 1-x > oxide, M comprises at least one of Li or rare earth elements; and x is in a range of 0.01 to 0.4. The material prepared by the preparation method disclosed by the invention can obviously improve the antibacterial property accidentally.

Description

Technical Field

[0001] The invention belongs to the preparation of antibacterial materials, and in particular to the field of magnesium oxide modified antibacterial materials. Background Art

[0002] Harmful microorganisms, especially common bacteria such as Escherichia coli and Helicobacter pylori, have a significant impact on human normal life and health. Therefore, solving the adverse effects of harmful microorganisms on human normal life has become a hot topic in today's society and a difficult problem that needs to be solved urgently. In this context, antibacterial materials have entered the public's field of vision and quickly become the focus of attention. The development of new, safe, environmentally friendly and effective antibacterial materials and how to achieve large-scale production and utilization of new antibacterial materials in industry have become hot topics.

[0003] As an emerging inorganic antibacterial material, MgO has entered people's field of vision and gradually become a hot spot in the research of antibacterial materials due to its advantages such as environmental friendliness, low cost and non-toxicity. And as the world's largest magnesium producing country, a large amount of magnesium ore resources cannot be effectively utilized after mining. The development of magnesium oxide antibacterial materials can not only solve the problem of lack of new antibacterial materials needed by society, but also help to increase the value of excessively accumulated magnesium ore. However, compared with traditional inorganic antibacterial materials, such as Ag-based materials, photocatalytic antibacterial materials TiO2, ZnO, etc., magnesium oxide materials have two disadvantages: on the one hand, the antibacterial performance of pure magnesium oxide is weak, and it is necessary to consider whether the addition of large doses of antibacterial materials will affect the product during the application process; on the other hand, although there are already enhanced magnesium oxide materials, the production cost is high and the process is complicated, which affects the economic benefits of the product. Therefore, it is necessary to develop a magnesium oxide material that has both high antibacterial performance and a production method close to industrialization.

[0004] In view of the problem that the antibacterial activity of magnesium oxide is not ideal, there are some improvement schemes in the prior art. For example, the Chinese patent document with publication number CN116463103A discloses an antibacterial and mildew-proof sealant and a preparation method thereof, and specifically discloses a Zn, Ce and Cu co-doped MgO. In addition, it also discloses a preparation method of calcining the raw materials of zinc source, cerium source, copper source, magnesium source and PEG400 at 450-550°C. In addition, the US patent document with publication number US20220279794A1 also discloses a co-doped magnesium oxide nanocomposite composition. The Chinese patent document with publication number CN112088897A discloses a nano-magnesium oxide inorganic antibacterial agent and a preparation method thereof, which specifically records the preparation process of calcining lithium salt, magnesium salt and complexing agent.

[0005] In summary, in order to solve the problem of unsatisfactory antibacterial performance of magnesium oxide, the existing main idea is to dope it with elements, but this method is difficult to further improve its antibacterial performance and efficiency, especially for difficult-to-treat Gram-negative bacteria, its antibacterial ability and efficiency need to be improved. Summary of the invention

[0006] In view of the problem that the antibacterial efficiency and effect of the existing magnesium oxide-based antibacterial materials are not ideal, especially it is difficult to show high antibacterial activity in Gram-negative bacteria, the first object of the present invention is to provide an oxygen-deficient wrinkle M x Mg 1-x The preparation method of oxide antibacterial material aims to prepare M with suitable oxygen defect wrinkle morphology and excellent antibacterial efficiency and effect. x Mg 1-x Oxide antibacterial material.

[0007] The second object of the present invention is to provide oxygen defect wrinkles M prepared by the preparation method x Mg 1-x Oxide antibacterial materials and their applications.

[0008] The third object of the present invention is to provide a method comprising the oxygen defect wrinkles M x Mg 1-x Antibacterial preparation of oxide antibacterial materials.

[0009] The antibacterial activity and antibacterial efficiency of existing magnesium oxide-based antibacterial materials are not ideal, especially for Gram-negative bacteria that are difficult to inhibit, their antibacterial efficiency and effect are even more unsatisfactory. Although the existing doping ideas can improve their antibacterial activity to a certain extent, for Gram-negative bacteria, the antibacterial efficiency and effect of modified materials are still not ideal. In view of this problem, the present invention has been studied in depth and provides the following improvement scheme:

[0010] An oxygen-deficient fold x Mg 1-x The preparation method of the oxide antibacterial material comprises obtaining a metal solution (also called a metal salt solution) in which a Mg source and a M source are dispersed, then atomizing the solution to obtain metal raw material particles (also called precursor particles), and then calcining the metal raw material particles in an oxygen-free atmosphere at a temperature of 500 to 1000° C. to obtain the oxygen-deficient wrinkled M x Mg 1-x Oxide antibacterial materials;

[0011] The M x Mg 1-x In the oxide, the M includes at least one of Li and rare earth elements; and x is 0.01 to 0.4.

[0012] Different from the conventional doping process that requires the assistance of organic matter, the present invention directly atomizes the metal solution without adding conventional carbon source, and further performs a subsequent calcination process in an oxygen-free atmosphere, so that gradient oxygen defects can be unexpectedly constructed on the surface, and not only that, the particles can also shrink to form a suitable wrinkled surface. The present invention's research shows that the material prepared by the preparation method can unexpectedly significantly improve the antibacterial performance, especially for difficult-to-treat Gram-negative bacteria, and can also show excellent short-term and high-efficiency antibacterial activity.

[0013] In the present invention, the Mg source and the M source are water-soluble salts of the respective metal elements, for example, at least one of an inorganic acid salt and an acetate salt.

[0014] Preferably, the rare earth element comprises at least one of Ce and La. Most preferably, the M is Li. Studies of the present invention show that the preferred M, combined with the process of the present invention, helps to further achieve synergy and can further optimize the antibacterial activity of the material against Gram-negative bacteria in a short time.

[0015] Preferably, the x is 0.05 to 0.2, and can further be 0.1 to 0.15. The present invention studies show that under the preferred x, it is combined with the process of the present invention to help further achieve synergy and further optimize the antibacterial activity of the material against Gram-negative bacteria in a short time.

[0016] In the present invention, the air inlet temperature of the atomization treatment is 180-240° C., and the air outlet temperature is 100-160° C. Further, the air inlet temperature of the atomization treatment is 200-240° C., and the air outlet temperature is 100-120° C.

[0017] Preferably, the particle size of the metal raw material particles is 1 to 5 μm.

[0018] In the present invention, the oxygen-free atmosphere is at least one of nitrogen and an inert gas, such as Ar.

[0019] In the present invention, the temperature of the first stage calcination may be 550 to 800°C, more preferably 600 to 700°C.

[0020] In the present invention, the holding time at the first stage calcination temperature is 2 to 6 hours, preferably 4 to 6 hours.

[0021] Preferably, after the first calcination, a second calcination is performed in an oxygen-containing atmosphere at a temperature above 300°C, preferably above 350°C, to obtain the oxygen defect wrinkle M x Mg 1-xOxide antibacterial material. The present invention shows that the subsequent calcination treatment of the product after the first stage of calcination in an oxygen-containing atmosphere can unexpectedly further optimize the deep antibacterial ability of the prepared material against Gram-negative bacteria.

[0022] In the present invention, the temperature of the second stage calcination is 350-450°C.

[0023] In the present invention, the holding time at the second calcination temperature is 1 to 4 hours, preferably 1 to 2 hours.

[0024] The present invention also provides oxygen defect wrinkle M prepared by the preparation method x Mg 1-x Oxide antibacterial material.

[0025] The preparation method described in the present invention can give the prepared material special physical and chemical characteristics, and the material with the characteristics prepared by the preparation method can unexpectedly and significantly enhance the antibacterial performance, especially for Gram-negative bacteria that are difficult to inhibit, and it can also obtain excellent antibacterial activity in a short time.

[0026] The oxygen defect wrinkle M of the present invention x Mg 1-x The oxide antibacterial material is black-gray or gray-white in color, and the particle size ranges from 10nm to 1μm.

[0027] The present invention also provides an oxygen defect wrinkle M prepared by the preparation method. x Mg 1-x Application of oxide antibacterial materials as antibacterial active ingredients for the preparation of antibacterial products that inhibit microorganisms;

[0028] Preferably, the microorganism is a bacterium, preferably a Gram-positive bacterium and / or a Gram-negative bacterium; more preferably a Gram-negative bacterium.

[0029] The present invention also provides an antibacterial product, which contains the oxygen-deficient wrinkled M prepared by the preparation method of the present invention. x Mg 1-x Oxide antibacterial material, and / or through the oxygen defect folds M x Mg 1-x Oxide antibacterial materials are prepared.

[0030] In the antibacterial product, the oxygen-deficient wrinkles M x Mg 1-x The content of the oxide antibacterial material can be reasonably adjusted as needed.

[0031] Beneficial Effects

[0032] The present invention directly atomizes the metal solution without adding any conventional carbon source, and further performs a subsequent calcination treatment in an oxygen-free atmosphere, which can unexpectedly construct gradient oxygen defects on the surface. Not only that, it can also achieve particle shrinkage to form a suitable wrinkled surface.

[0033] The present invention shows that the material prepared by the preparation method can significantly improve the antibacterial performance, especially can obtain excellent antibacterial activity against Gram-negative bacteria in a short time. In particular, the combination of M species, x and calcination mechanism helps to further optimize the antibacterial activity of the prepared material against Gram-negative bacteria. BRIEF DESCRIPTION OF THE DRAWINGS

[0034] Figure 1 These are the SEM overall image of the powder precursor material during the preparation process in Comparative Example 1 and the local magnified image of the material.

[0035] Figure 2 These are the overall SEM images of the metal-doped magnesium oxide material and the undoped magnesium oxide material prepared in Comparative Example 1, Example 1, and Example 2.

[0036] Figure 3 These are SEM magnified images of the metal-doped magnesium oxide material and the undoped magnesium oxide material prepared in Comparative Example 1, Example 1, and Example 2, as well as local magnified images of the materials.

[0037] Figure 4 The metal-doped magnesium oxide material prepared in Example 1, Example 1 and Example 2 and the undoped magnesium oxide material are compared. x X-ray diffraction pattern and single peak magnification.

[0038] Figure 5 The metal-doped magnesium oxide material prepared in Example 1, Example 1 and Example 2 and the undoped magnesium oxide material are compared. XPS O element peak diagram of each material in the analysis.

[0039] Figure 6 This is an experimental diagram of the minimum inhibitory concentration of the metal-doped magnesium oxide material and the undoped magnesium oxide material prepared in Comparative Example 1, Example 1, and Example 2. DETAILED DESCRIPTION

[0040] The specific implementation of the present invention will be described clearly and completely below in conjunction with the accompanying drawings. The pure magnesium oxide material used in the implementation of the present invention is a commercially available nano magnesium oxide material.

[0041] Comparative Example 1

[0042] Step 1. Dissolve magnesium acetate in 500 mL of deionized water and sonicate until it is completely dissolved to form a uniform and clear solution.

[0043] Step 2. Spray drying to prepare a powder precursor: first, evenly flow deionized water into the spray dryer at a constant flow rate, set the spray dryer equipment parameters to an inlet air temperature of 220°C, adjust the spray air flow, wait for the outlet air temperature to be constant, at which time the outlet air temperature should be greater than 100°C, and evenly flow the magnesium acetate solution in step 1 into the spray dryer at a constant flow rate. After the solution completely enters the spray dryer, turn off the heater, wait for the equipment temperature to drop to room temperature, then turn off the equipment, and remove the collector to collect the precursor powder.

[0044] Step 3. Primary calcination: calcine the precursor powder at 600° C. for 4 h in an argon atmosphere, and after the calcination is completed, take out the product and grind it to obtain an intermediate product.

[0045] Step 4. Secondary calcination: The intermediate product is placed in a muffle furnace and calcined at 400° C. for 2 h for secondary calcination. After calcination, pure magnesium oxide powder (labeled as MgO) is obtained.

[0046] Example 1

[0047] Compared with Comparative Example 1, the only difference is that in step 1, lithium acetate is added, and the molar ratio of lithium to magnesium is 1:9. Other operations and parameters are the same as those in Example 1. The obtained material is marked as LiMgO (also known as Li 0.1 Mg 0.9 oxide).

[0048] Example 2

[0049] Compared with Comparative Example 1, the only difference is that in step 1, cerium nitrate hexahydrate is added, and the molar ratio of Ce to magnesium is 1:9. Other operations and parameters are the same as those in Example 1. The obtained material is marked as CeMgO (also called Ce 0.1 Mg 0.9 oxide).

[0050] Example 3

[0051] Compared with Example 1, the only difference is that the molar ratio of lithium to magnesium in step 1 is changed to 1:19, and the other operations and parameters are the same as those in Example 1. The obtained material is marked as LiMgO (0.05) (also known as Li 0.05 Mg 0.95 oxide).

[0052] Example 4

[0053] Compared with Comparative Example 1, the only difference is that lanthanum nitrate hexahydrate is added, and the molar ratio of La to magnesium is 1:9, and the other operations and parameters are the same as those in Example 1. The obtained material is marked as LaMgO (also known as La0.1Mg0.9 oxide).

[0054] Example 5

[0055] Compared with Example 1, the only difference is that the atomization air inlet temperature is 240°C, the temperature of the first stage calcination is 700°C, the time is 5 hours, and the time of the second stage calcination is 450°C, the time is 1 hour. Other operations and parameters are the same as in Example 1. The obtained material is marked as LiMgO (700).

[0056] Example 6

[0057] Compared with Example 1, the only difference is that the second stage calcination is not performed, and the other operations and parameters are the same as those of Example 1. The obtained material is marked as LiMgO (single calcination).

[0058] Comparative Example 2

[0059] Compared with Example 1, the only difference is that the raw material is not sprayed, but directly evaporated and desolventized to obtain a precursor, and then a subsequent sintering treatment is performed. Other operations and parameters are the same as Example 1. The obtained material is marked as LiMgO-2.

[0060] Comparative Example 3

[0061] Compared with Example 2, the only difference is that the raw material is not sprayed, but directly evaporated and desolventized to obtain a precursor, and then a subsequent sintering treatment is performed. Other operations and parameters are the same as those in Example 1. The obtained material is marked as CeMgO-2.

[0062] Comparative Example 4

[0063] Compared with Example 1, the only difference is that the atmosphere of the first stage calcination is air, and the other operations and parameters are the same as those of Example 1. The obtained material is marked as LiMgO (air).

[0064] Comparative Example 5

[0065] Compared with Comparative Example 1, the only difference is that in step 1, zinc nitrate nonahydrate is added, and the molar ratio of Zn to magnesium is 1:9. Other operations and parameters are the same as those in Example 1. The obtained material is marked as ZnMgO (also known as Zn 0.1 Mg 0.9 oxide).

[0066] Test 1:

[0067] The scanning electron microscope images of Comparative Example 1, Example 1, Example 2 and the powder precursor of the present invention are as follows: Figure 1 and Figure 2 As shown, Figure 1 SEM image of the powder precursor. Figure 2 The SEM overall images of Comparative Example 1, Example 1 and Example 2 are shown in FIG. Figure 3 These are the SEM magnified images and local magnified images of the materials of Comparative Example 1, Example 1 and Example 2, wherein a is the pure magnesium oxide prepared in Comparative Example 1, b is the LiMgO prepared in Example 1, and c is the CeMgO prepared in Example 2.

[0068] pass Figure 1 It can be seen that the prepared powder precursor is a spherical micron-sized particle material with wrinkles on the surface. Figure 2 , 3 From the image, we can see that after two calcinations, the precursor powder particles began to shrink inward due to the high temperature during the calcination process, the particle diameter began to decrease and slight agglomeration occurred. The material after calcination is still spherical particles but the surface is rougher than that of the precursor particles.

[0069] Test 2:

[0070] This comparative example 1, embodiment 1, embodiment 2 x The X-ray diffraction results are as follows Figure 4 As shown, a is pure magnesium oxide prepared in Comparative Example 1, b is LiMgO prepared in Example 1, and c is CeMgO prepared in Example 2.

[0071] In order to compare the crystal phase of the antibacterial material before and after metal doping, the material was x X-ray diffraction. Figure 4 It can be seen that after comparison with the standard card, pure magnesium oxide perfectly matches the standard card, indicating that the magnesium oxide prepared according to the claimed method has a stable crystal form and high purity. At the same time, it is found that the magnesium oxide material loaded with lithium can also perfectly match the standard card, indicating that the metal loading does not cause a significant change in the overall crystal phase of the material, but after amplifying a single peak, it is found that the peak shape is slightly shifted, indicating that the metal has been doped into the magnesium oxide and replaced with the magnesium element. The purpose of preparing metal-doped magnesium oxide antibacterial materials is achieved.

[0072] Test 3:

[0073] The XPS test results of Comparative Example 1, Example 1 and Example 2 are as follows Figure 5 As shown, a is the pure magnesium oxide prepared in Comparative Example 1, b is the LiMgO prepared in Example 1, and c is the CeMgO prepared in Example 2.

[0074] The XPS test is performed to verify whether the number of surface oxygen vacancies / defects is improved.

[0075] The number of surface oxygen vacancies / defects is mainly determined by narrow scanning of the O element and the proportion of different peaks after peak separation. According to literature research, the binding energy of 529.3-529.8eV is lattice oxygen, and the binding energy of 531.2-531.6eV is absorbed oxygen. As the number of surface oxygen vacancies increases, the number of external oxygen atoms increases.

[0076] It is absorbed on the surface of the material, and the absorbed oxygen content increases accordingly. Therefore, the higher the absorbed oxygen content, the lower the surface oxygen vacancy.

[0077] The more bits there are. Figure 5 It can be seen that the absorbed oxygen content increases after metal doping, indicating that metal doping effectively increases the number of oxygen vacancies on the magnesium oxide surface.

[0078] Test 4:

[0079] Antibacterial performance test:

[0080] Metal doping can effectively improve the antibacterial properties of magnesium oxide by improving the antibacterial properties. Gram-negative bacteria (E. coli, ATCC8739) were selected as the object in the test. The minimum inhibitory concentration (MIC) and antibacterial rate of comparative example 1, example 1, and example 2 were tested, and the performance difference between the antibacterial properties of the magnesium oxide material before and after metal doping prepared by the present invention was obtained, reflecting the effectiveness of the invention. The specific experimental steps are as follows:

[0081] Step 1. Bacterial culture: The E. coli strain was cultured in LB medium at 37°C for 4 to 5 hours until the absorbance of the bacterial suspension at 600nm reached 1.3 to 1.4. In this state, the bacterial growth reached the logarithmic phase and showed the highest cell activity. It should be noted that all glassware and culture media used in the test have been sterilized at a high temperature and pressure of 121°C.

[0082] Step 2. Minimum inhibitory concentration (MIC) test: Add different concentrations of antibacterial materials to LB liquid (10 ml) culture medium, and then add 0.2 ml of a logarithmic phase concentration of 10 6 The mixture was incubated at 37°C for 24 hours, and the minimum inhibitory concentration was determined by the concentration of the sample in the bottle that remained clear after incubation. Figure 6 shown.

[0083] Step 3. Antibacterial rate test:

[0084] Blank control group setting: 1mL original bacterial solution (bacterial solution concentration is about 10 8 cfu / mL) were added into 10 mL of normal saline to obtain a blank control group.

[0085] Antibacterial test group: 1mL of original bacterial solution (bacterial solution concentration is about 10 8 cfu / mL) were added to 9 mL of normal saline. Then, 4 mg of different test samples were added, and the sample concentration was 400 μg ml -1 After incubation at 37°C for 15 minutes, take 100 μL and spread it evenly on the agar plate. Incubate at 37°C for 24 hours and calculate the inhibition rate. The inhibition rate calculation formula is as follows:

[0086]

[0087] It should be noted that Ar represents the inhibition rate, A represents the count of live bacteria in the control group, and B represents the count of live bacteria in the experimental group.

[0088] according to Figure 6 The experimental results show that after metal doping, the minimum inhibitory concentration of the antibacterial material decreases, which means that the antibacterial properties of the magnesium oxide material are significantly improved after metal doping. According to Table 2, when the material concentration is the same, the metal-doped magnesium oxide material shows a higher antibacterial rate than the pure magnesium oxide material, indicating that the antibacterial properties of the magnesium oxide material after metal doping are better. Among them, the metal lithium-doped magnesium oxide material shows an efficient antibacterial rate of more than 99.99% after 15 minutes of antibacterial contact, while the antibacterial rate of pure magnesium oxide is only 67.86%, showing the superior antibacterial properties of the metal-doped magnesium oxide antibacterial material.

[0089] Table 1 Minimum inhibitory concentration (MIC) test results

[0090]

[0091] It should be noted that O represents turbidity, i.e. bacterial growth, and x represents clarity, i.e. sterile growth.

[0092] Table 2 Bacterial counts of different samples after antibacterial test

[0093]

[0094]

[0095] In summary, the present invention directly atomizes the metal solution without adding a conventional carbon source, and further performs a subsequent first stage calcination treatment in an oxygen-free atmosphere, and in particular, further performs a subsequent second stage calcination in an oxygen-containing atmosphere, so that gradient oxygen defects can be unexpectedly constructed on the surface, and not only that, the particles can also shrink to form a suitable wrinkled surface. The present invention's research shows that the material prepared by the preparation method can unexpectedly significantly improve the antibacterial performance, especially can obtain excellent antibacterial activity against Gram-negative bacteria in a short time.

[0096] The above are only preferred embodiments of the present invention, and only describe the implementation methods of the present invention. They do not limit the patent scope of the present invention. All equivalent structural changes made by using the contents of the present invention specification and drawings under the technical concept of the present invention, or directly / indirectly applied in other related technical fields are included in the patent protection scope of the present invention.

Claims

1. An oxygen defect wrinkle M x Mg 1-x The method for preparing an oxide antibacterial material is characterized in that: A metal solution containing a Mg source and a M source is obtained, and then the metal solution is atomized to obtain metal raw material particles. The metal raw material particles are then calcined in an oxygen-free atmosphere at a temperature of 500 to 1000° C. to obtain the oxygen-deficient wrinkled M x Mg 1-x Oxide antibacterial materials; The M x Mg 1-x In the oxide, the M includes at least one of Li and rare earth elements; and x is 0.01 to 0.

4.

2. The oxygen-deficient wrinkle M according to claim 1 x Mg 1-x The method for preparing an oxide antibacterial material is characterized in that: The Mg source and the M source are water-soluble salts of the respective metal elements, preferably at least one of an inorganic acid salt and an acetate; Preferably, the rare earth element comprises at least one of Ce and La; More preferably, the M comprises Li.

3. The oxygen-deficient wrinkle M according to claim 1 x Mg 1-x The method for preparing an oxide antibacterial material is characterized in that: The inlet air temperature of the atomization treatment is 180-240°C, and the outlet air temperature is 100-160°C; preferably, the inlet air temperature of the atomization treatment is 200-240°C, and the outlet air temperature is 100-120°C; Preferably, the particle size of the metal raw material particles is 1 to 5 μm.

4. The oxygen-deficient wrinkle M according to claim 1 x Mg 1-x The method for preparing an oxide antibacterial material is characterized in that: The oxygen-free atmosphere is at least one of nitrogen and an inert gas; Preferably, the inert gas comprises Ar gas.

5. The oxygen-deficient wrinkle M according to claim 1 x Mg 1-x The method for preparing an oxide antibacterial material is characterized in that: The temperature of the first stage calcination is 550-800°C, preferably 600-700°C; Preferably, the holding time at the first calcination temperature is 2 to 6 hours, preferably 4 to 6 hours.

6. The oxygen-deficient wrinkle M according to claim 1 x Mg 1-x The method for preparing an oxide antibacterial material is characterized in that: After the first calcination, a second calcination is performed in an oxygen-containing atmosphere at a temperature above 300°C, preferably above 350°C, to obtain the oxygen defect wrinkles M x Mg 1-x Oxide antibacterial material.

7. The oxygen-deficient wrinkle M according to claim 6 x Mg 1-x The method for preparing an oxide antibacterial material is characterized in that: The temperature of the second stage calcination is 350-450°C; Preferably, the holding time at the second calcination temperature is 1 to 4 hours, preferably 1 to 2 hours.

8. An oxygen-deficient wrinkle M obtained by the preparation method according to any one of claims 1 to 7 x Mg 1-x Oxide antibacterial material.

9. An oxygen-deficient wrinkle M obtained by the preparation method according to any one of claims 1 to 7 x Mg 1-x The application of oxide antibacterial materials is characterized by: It is used as an antimicrobial active ingredient to prepare antimicrobial products that inhibit microorganisms; Preferably, the microorganism is a bacterium, preferably a Gram-positive bacterium and / or a Gram-negative bacterium; more preferably a Gram-negative bacterium.

10. An antibacterial product, characterized in that: Adding oxygen defect wrinkles M prepared by the preparation method according to any one of claims 1 to 7 x Mg 1-x Oxide antibacterial material, and / or through the oxygen defect folds M x Mg 1-x Oxide antibacterial materials are prepared.

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